AMD 070 hydrochloride synthesis
- Product Name:AMD 070 hydrochloride
- CAS Number:880549-30-4
- Molecular formula:C21H28ClN5
- Molecular Weight:385.94
558447-26-0
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880549-30-4
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Yield:880549-30-4 98%
Reaction Conditions:
with hydrogenchloride in methanol;water at 70; for 1 h;
Steps:
1
In a 50 mL round-bottom flask, the compound of the Formula I (0.258 g, 0.738 mmol) was dissolved in reagent grade methanol (5 mL) to generate a colorless solution. The solution was diluted with water (15 mL) and then aqueous hydrochloric acid (0.0978 N, 7.56 mL, 1 equiv.) was added in one portion. The resulting mixture was stirred at 70° C. for one hour. The solvents were removed in vacuo and the resulting clear glass residue was dissolved in water (5 mL) and transferred to a 30 mL plastic bottle. The solution was frozen with liquid nitrogen and then lyophilized over two days to yield a fluffy white solid which was subsequently ground to a fine white powder of the hydrochloride salt of the compound of the Formula I (0.280 g, 98%). HPLC: 98% (>99% ee). GC: CH2Cl2 (5 ppm), EtOAc (4 ppm), MeOH (0 ppm). Anal. Calcd. for C21H27N5.1.1 HCl.1.4H2O: C, 60.81; H, 7.51; N, 16.88; Cl, 9.40. Found: C, 60.80; H, 7.20; N, 16.81; Cl, 9.40.
References:
US2006/69122,2006,A1 Location in patent:Page/Page column 5
163798-87-6
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369656-57-5
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880549-30-4
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